CN101914119A - Preparation method of konjak ceramide reference sample - Google Patents
Preparation method of konjak ceramide reference sample Download PDFInfo
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- CN101914119A CN101914119A CN2010102541475A CN201010254147A CN101914119A CN 101914119 A CN101914119 A CN 101914119A CN 2010102541475 A CN2010102541475 A CN 2010102541475A CN 201010254147 A CN201010254147 A CN 201010254147A CN 101914119 A CN101914119 A CN 101914119A
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- methanol
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Abstract
The invention discloses a preparation method of a konjak ceramide reference sample. The preparation method mainly comprises the following steps: (1) preparing a reference sample by RP-C18 gel column chromatography: packing the column by a wet process, loading a sample by a wet process, and effectively separating the impurities from ceramide by using the RP-C18 gel column according to the polar difference of the separated substances; and (2) collecting out-flowing components when the volume ratio of water to methanol in the eluent is 2:8 to 5:5, wherein the RP-C18 gel column chromatography adopts gradient elution, and the eluent is prepared from water and methanol in different ratios. The invention has the advantages of advanced technique, simple and convenient operation, high yield and low production cost.
Description
Technical field
The present invention relates to a kind of preparation method of standard specimen, be specifically related to a kind of preparation method of konjak ceramide reference sample.
Background technology
Ceramide is the integral part of cytolemma, has following biological function: 1, ceramide combines with glucoside and forms the schwann's sheath glycosides, is present in eukaryotic cytolemma such as animal and plant, participates in cell function; 2. regulate the effect of cell growth variability; 3. cell death inducing; 4. adjusting protein excretion; 5. the effect in inflammation; 6. has good water retention etc.The ceramide type material is the macromolecular compound of a class, and the molecular structure complexity if there is not standard model, just can't detect content, also just can't prove to have or not ceramide in the extract, and whether extraction process is effective.The content detection of ceramide, though the detection method of animal nerve acid amides is arranged, standard specimen is easily bought, but for the vegetative nerve acid amides is other the same thing, standard specimen is hard to buy, and especially konjak ceramide not only can't buy standard specimen, and simultaneously relevant its structure, molecular weight etc. are a blank fully.
The contriver has carried out long-term a large amount of research to the method for extracting ceramide from konjaku, has finished the technical study of extracting ceramide from konjaku at present, and has applied for patent in China, and number of patent application is CN200910263528.7.The present invention is on this basis, the further research that konjak ceramide is carried out, konjak ceramide based on disclosed method preparation in the above-mentioned patent application, identify by purifying and structure, prepare the standard specimen of konjak ceramide, for this area provides the research basis to the further utilization of konjak ceramide.
Summary of the invention
The invention provides a kind of preparation method of konjak ceramide reference sample, realize by following steps:
Step (1), employing RP-C
18Silica gel column chromatography prepares standard specimen: by wet method dress post, sample on the wet method according to the polarity difference of institute's separate substance, adopts RP-C
18Silicagel column makes impurity effectively be separated with ceramide.
Step (2), effusive component: RP-C when collecting elutriant volume ratio was to 5: 5 volume ratios of water-methanol from 2: 8 by water-methanol
18Silica gel column chromatography adopts gradient elution, and elutriant is that water-methanol is prepared by different ratios.
Further technical scheme is the described RP-C of step (1)
18Silica gel column chromatography, eluent flow rate are 1.0ml/min, and every 5ml collects once.
Further technical scheme is the described RP-C of step (2)
18Silica gel column chromatography elutriant graded is: water-methanol is 1: 9-8: 2 volume ratios.
Further technical scheme is the described RP-C of step (2)
18When silica gel column chromatography prepares, collect when volume ratio was to 5: 5 volume ratios of water-methanol from 2: 8 in water-methanol and to obtain four standard specimens of konjak ceramide.
The invention provides the preparation method of konjak ceramide reference sample, konjak ceramide is carried out purifying and structural analysis evaluation, the standard specimen that has prepared konjak ceramide is laid a good foundation for the further utilization to konjak ceramide, has very actual economic benefit and social benefit.
Embodiment
A kind of preparation method of konjak ceramide reference sample is that the konjak ceramide composition behind the purifying is carried out RP-C
18Silica gel column chromatography separates, and water-methanol gradient elution, eluent flow rate are 1.0ml/min, and every 5ml collects once.5: 5 from 2: 8 volume ratios to water-methanol volume ratios of water-methanol collect chemical compounds I, II, III, IV.
Chemical compounds I, II, III, IV are white unformed pulverulent solids.Respectively chemical compounds I, II, III, IV are carried out structure elucidation, obtain as drawing a conclusion: the ESI-MS of chemical compounds I, II, III, IV shows m/z 736.80,746.72,792.81,820.70 respectively, its
1HNMR
13CNMR HMBC
1H-
1H COSY spectrogram shows that chemical compounds I, II, III, IV are following structure:
Wherein, the n value of chemical compounds I, II, III, IV correspondence is respectively 11,13,15,19.
The title of the konjak ceramide reference material of four kinds of compound correspondences is respectively:
1-O-β-D-Glucopyranose-(2S, 3R, 4E, 8Z)-2-N-[(2 ' R)-2-hydroxyl-palmitoyl ammonia amine]-4,8 ten eight carbon diene;
1-O-β-D-Glucopyranose-(2S, 3R, 4E, 8Z)-2-N-[(2 ' R)-2-hydroxyl-octadecanoyl ammonia amine]-4,8 ten eight carbon diene;
1-O-β-D-Glucopyranose-(2S, 3R, 4E, 8Z)-2-N-[(2 ' R)-2-hydroxyl-20 phosphinylidyne ammonia amine]-4,8 ten eight carbon diene;
1-O-β-D-Glucopyranose-(2S, 3R, 4E, 8Z)-2-N-[(2 ' R)-2-hydroxyl-22 phosphinylidyne ammonia amine] phosphinylidyne ammonia amine]-4,8 ten eight carbon diene.
Claims (4)
1. the preparation method of a konjak ceramide reference sample is characterized in that realizing by following steps:
Step (1), employing RP-C
18Silica gel column chromatography prepares standard specimen: by wet method dress post, sample on the wet method according to the polarity difference of institute's separate substance, adopts RP-C
18Silicagel column makes impurity effectively be separated with ceramide;
Step (2), effusive component: RP-C when collecting elutriant volume ratio was to 5: 5 volume ratios of water-methanol from 2: 8 by water-methanol
18Silica gel column chromatography adopts gradient elution, and elutriant is that water-methanol is prepared by different ratios.
2. the preparation method of konjak ceramide reference sample according to claim 1 is characterized by the described RP-C of step (1)
18Silica gel column chromatography, eluent flow rate are 1.0ml/min, and every 5ml collects once.
3. the preparation method of konjak ceramide reference sample according to claim 1 is characterized by the described RP-C of step (2)
18Silica gel column chromatography elutriant graded is: water-methanol is 1: 9-8: 2 volume ratios.
4. the preparation method of konjak ceramide reference sample according to claim 1 is characterized by the described RP-C of step (2)
18When silica gel column chromatography prepares, collect when volume ratio was to 5: 5 volume ratios of water-methanol from 2: 8 in water-methanol and to obtain four standard specimens of konjak ceramide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102541475A CN101914119A (en) | 2010-08-16 | 2010-08-16 | Preparation method of konjak ceramide reference sample |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102541475A CN101914119A (en) | 2010-08-16 | 2010-08-16 | Preparation method of konjak ceramide reference sample |
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| CN101914119A true CN101914119A (en) | 2010-12-15 |
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| CN2010102541475A Pending CN101914119A (en) | 2010-08-16 | 2010-08-16 | Preparation method of konjak ceramide reference sample |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351730A (en) * | 2011-10-22 | 2012-02-15 | 恩施清江生物工程有限公司 | Method for preparing ceramide from konjac fly powder |
-
2010
- 2010-08-16 CN CN2010102541475A patent/CN101914119A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351730A (en) * | 2011-10-22 | 2012-02-15 | 恩施清江生物工程有限公司 | Method for preparing ceramide from konjac fly powder |
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Application publication date: 20101215 |